反应详情

温度

40 °C

To a solution of (2S,5R)-2-[2-(2-chloro-phenyl)-ethyl]-5-isopropyl-3,6-dimethoxy-2-methyl-2,5-dihydro-pyrazine (1.22 g, 3.62 mmol) in acetonitrile (12 ml) were added water (4 ml) and trifluoroacetic acid (2 ml). The mixture was stirred overnight at 40° C. Saturated ammonium chloride solution was added and the mixture was extracted with dichloromethane three times. The combined organic layers were dried (MgSO4), filtered and evaporated. The residue was purified by column chromatography (SiO2, EtOAc/MeOH=95:5 to yield a colorless oil, (0.46 g, 52%); MS (ISP): 242.1; 244.1 ((M+H)+.).

1. extractionthe mixture was extracted with dichloromethane three times
2. dry with materialThe combined organic layers were dried (MgSO4)
3. filtrationfiltered
4. customevaporated
5. customThe residue was purified by column chromatography (SiO2, EtOAc/MeOH=95:5
6. customto yield a colorless oil, (0.46 g, 52%)